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Title: Imaging Unstained Synthetic Polymer Crystals and Defects on Atomic Length Scales Using Cryogenic Electron Microscopy

Abstract

Properties of soft crystalline materials such as synthetic polymers are governed by locations of constituent atoms. Determining atomic-scale structures in these materials is difficult because they degrade rapidly when studied by electron microscopy, and techniques such as x-ray scattering average over volumes much larger than coherent blocks of the unit cells. We obtained cryo-electron microscopy images of self-assembled nanosheets of a peptoid polymer, made by solid-phase synthesis, in which we see a variety of crystalline motifs. A combination of crystallographic and single particle methods, developed for cryo-electron microscopy of biological macromolecules, was used to obtain high resolution images of the crystals. Individual crystals contain grains that are mirror images of each other with concomitant grain boundaries. We have used molecular dynamic simulations to build an atomic model of the crystal structure to facilitate the interpretation of electron micrographs. Direct visualization of crystalline grains and grain boundaries on atomic length scales represents a new level of information for the polymer field.

Authors:
ORCiD logo [1]; ORCiD logo [2];  [3];  [4];  [5];  [4]; ORCiD logo [4]; ORCiD logo [2]; ORCiD logo [6]
+ Show Author Affiliations
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). College of Chemistry
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Foundry; Duke Univ., Durham, NC (United States). Dept. of Chemistry
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Foundry
  5. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Foundry; Univ. of California, Berkeley, CA (United States). Dept. of Materials Science and Engineering
  6. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Biophysics and Integrated Bioimaging Division
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division
OSTI Identifier:
1507257
Alternate Identifier(s):
OSTI ID: 1601193
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Macromolecules
Additional Journal Information:
Journal Volume: 51; Journal Issue: 19; Journal ID: ISSN 0024-9297
Publisher:
American Chemical Society
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; peptoids; structure; cryo-EM; polymers, defects

Citation Formats

Jiang, Xi, Greer, Douglas R., Kundu, Joyjit, Ophus, Colin, Minor, Andrew M., Prendergast, David, Zuckermann, Ronald N., Balsara, Nitash P., and Downing, Kenneth H. Imaging Unstained Synthetic Polymer Crystals and Defects on Atomic Length Scales Using Cryogenic Electron Microscopy. United States: N. p., 2018. Web. doi:10.1021/acs.macromol.8b01508.
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Jiang, Xi, Greer, Douglas R., Kundu, Joyjit, Ophus, Colin, Minor, Andrew M., Prendergast, David, Zuckermann, Ronald N., Balsara, Nitash P., & Downing, Kenneth H. Imaging Unstained Synthetic Polymer Crystals and Defects on Atomic Length Scales Using Cryogenic Electron Microscopy. United States. doi:10.1021/acs.macromol.8b01508.
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Jiang, Xi, Greer, Douglas R., Kundu, Joyjit, Ophus, Colin, Minor, Andrew M., Prendergast, David, Zuckermann, Ronald N., Balsara, Nitash P., and Downing, Kenneth H. Tue . "Imaging Unstained Synthetic Polymer Crystals and Defects on Atomic Length Scales Using Cryogenic Electron Microscopy". United States. doi:10.1021/acs.macromol.8b01508. https://www.osti.gov/servlets/purl/1507257.
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@article{osti_1507257,
title = {Imaging Unstained Synthetic Polymer Crystals and Defects on Atomic Length Scales Using Cryogenic Electron Microscopy},
author = {Jiang, Xi and Greer, Douglas R. and Kundu, Joyjit and Ophus, Colin and Minor, Andrew M. and Prendergast, David and Zuckermann, Ronald N. and Balsara, Nitash P. and Downing, Kenneth H.},
abstractNote = {Properties of soft crystalline materials such as synthetic polymers are governed by locations of constituent atoms. Determining atomic-scale structures in these materials is difficult because they degrade rapidly when studied by electron microscopy, and techniques such as x-ray scattering average over volumes much larger than coherent blocks of the unit cells. We obtained cryo-electron microscopy images of self-assembled nanosheets of a peptoid polymer, made by solid-phase synthesis, in which we see a variety of crystalline motifs. A combination of crystallographic and single particle methods, developed for cryo-electron microscopy of biological macromolecules, was used to obtain high resolution images of the crystals. Individual crystals contain grains that are mirror images of each other with concomitant grain boundaries. We have used molecular dynamic simulations to build an atomic model of the crystal structure to facilitate the interpretation of electron micrographs. Direct visualization of crystalline grains and grain boundaries on atomic length scales represents a new level of information for the polymer field.},
doi = {10.1021/acs.macromol.8b01508},
journal = {Macromolecules},
number = 19,
volume = 51,
place = {United States},
year = {2018},
month = {9}
}
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Journal Article:
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Publisher's Version of Record
DOI:  10.1021/acs.macromol.8b01508
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Cited by: 7 works
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Figures / Tables:

Figure 1 Figure 1: Chemical structure and EM characterization. A, Chemical structure of peptoid pNdc9–pNte9. B, TEM micrograph of pNdc9–pNte9 sheets. C, Cryogenic electron diffraction pattern of a vitrified hydrated pNdc9–pNte9 sheet; the brighter ring corresponds to gold 111 diffraction at 2.35Å, inset red circle indicates (1, 19) reflection at 2.3 Å.more » D, Cryo-EM micrograph (reversed contrast) of a vitrified hydrated pNdc9–pNte9 sheet; inset shows a Fourier filtered image. E, The Fourier transform of an image of a vitrified hydrated pNdc9–pNte9 sheet showing reflections and Thon rings due to the thin carbon support; red circle in inset indicates the (1, 19) reflection. F, Information in Fourier transform of image after correction for lattice distortions. The rings represent resolution of 2.0, 2.35, 4.5, and 24.5 Å, H and K indicate directions of lattice vectors, and red circle indicates the (1, 19) reflection. The squares indicate the signal-to-noise ratio of reflections: the larger the square is, the better the image quality (IQ).« less
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Works referencing / citing this record:

Design and preparation of organic nanomaterials using self‐assembled peptoids
journal, February 2019

Recent advances in crystallization and self‐assembly of polypeptoid polymers
journal, June 2019

  • Zeng, Guangjian; Qiu, Lu; Wen, Tao
  • POLYMER CRYSTALLIZATION, Vol. 2, Issue 3
  • DOI: 10.1002/pcr2.10065

Atomic-level engineering and imaging of polypeptoid crystal lattices
journal, October 2019

  • Xuan, Sunting; Jiang, Xi; Spencer, Ryan K.
  • Proceedings of the National Academy of Sciences, Vol. 116, Issue 45
  • DOI: 10.1073/pnas.1909992116
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